反应详情

To a suspension of perfluorooctanesulfonic acid potassium salt (24.64 g, 46.1 mmol) in water (150 ml) at room temperature under nitrogen was added dropwise triphenylsulfonium chloride (50% aqueous solution, 27.50 g) over 15 minutes. After stirring the suspension for 30 minutes, dichloromethane (75 ml) was added and the mixture stirred at room temperature for 20 hours. Additional dichloromethane (225 ml) was added and the layers separated. The organic layer was washed with water (5×125 ml) until the washings were neutral (pH 7 ). After drying (MgSO4 ), removal of the solvent in vacuo gave a viscous gum which was further dried by heating at 80°-90° C. for 84 hours under vacuum. In this way, triphenylsulfonium perfluorooctanesulfonate was isolated as a glassy solid (30.61 g).

1. stirringthe mixture stirred at room temperature for 20 hours
2. customthe layers separated
3. washThe organic layer was washed with water (5×125 ml) until the washings
4. customAfter drying
5. custom(MgSO4 ), removal of the solvent in vacuo
6. customgave a viscous gum which
7. customwas further dried
8. temperatureby heating at 80°-90° C. for 84 hours under vacuum